CN207786609U - A kind of organic chemical synthesis reactor of integration operation - Google Patents
A kind of organic chemical synthesis reactor of integration operation Download PDFInfo
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- CN207786609U CN207786609U CN201721750699.9U CN201721750699U CN207786609U CN 207786609 U CN207786609 U CN 207786609U CN 201721750699 U CN201721750699 U CN 201721750699U CN 207786609 U CN207786609 U CN 207786609U
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Abstract
The utility model is related to the organic chemical synthesis reactors of integration operation, including reaction bulb, reaction bottle cap, reaction bulb heating device, ultrasonic nebulizer, xenon lamp, thermometric and cooling device, extraction equipment, eluent device for formulating, chromatographic column separator and receiving bottle；Reaction bulb is placed at the top of reaction bulb and closed with reaction bulb；Reaction bulb heating device is placed in reaction bulb bottom and/or side；It is connected inside ultrasonic nebulizer and reaction bulb；Xenon lamp and thermometric and cooling device are through to from reaction bottle cap inside reaction bulb respectively；Extraction equipment is arranged in reaction bulb bottom and is connected with inside reaction bulb；Extraction equipment and eluent device for formulating are connected with chromatographic column separator respectively；Chromatographic column separator is connected with receiving bottle.The advantages of the utility model can carry out the separation of solid product, product liquid and gas-phase product and not only save the time of organic synthetic experiment but also reduce waste and the energy consume of reaction raw materials.
Description
Technical field
The utility model belongs to organic chemical synthesis technical field, is related to a kind of organic chemical synthesis reactor, especially relates to
And it is a kind of can integration operation organic chemical synthesis reactor.
Background technology
With the rapid development of chemical science and technology and the gradual maturation of organic chemical synthesis technology, organic synthesis can be from
Simple compound or element after chemical reaction anthropogenics, the 1830's have synthesized urea；After 19th century
Half hinge is at a variety of dyestuffs；DDT and organophosphorus insecticide, organosulfureous fungicide, herbicide etc. are synthesized the 1940s
Pesticide；It has synthesized 606 medicaments early 20th century, has synthesized more than 1,000 kinds of sulfonamides compound 30~forties, these organise
The synthesis and use for closing object play vital effect in daily life, industrial and agricultural production, life science etc..
Organic synthesis is to study its composition, structure, property and the premise of effect, and chemical synthesising technology develops over 100 years
Rapidly, what many new technologies were all successive is used for the synthesis of organic compound, for example, high―temperature nuclei, high-pressure synthesis, electrolysis conjunction
At, photosynthesis, phonosynthesis, microwave synthesis, plasma synthesis, synthesis in solid state, bio-mimetic syntheses etc..Wherein thermal synthesis technology and
Photosynthesis Technical comparing is common, is urgently required to the special purpose reactor for organic synthesis, existing photosynthesis device, heat
Synthesizer and pillar layer separation all are separated to use during the experiment, can lead to that the reaction time is long and operating process is numerous
It is miscellaneous, the waste of some unnecessary losses and resource is brought to experimentation.
With the continuous improvement and application of photosynthesis technology, microwave-assisted synthesis and traditional thermal synthesis technology, have
Machine synthesizer is moving to maturity step by step, and publication number is to provide a kind of knot in the utility model patent of CN204583168U
Structure is simple, safe to use, and the high organic synthesis microwave device of reaction efficiency can recycle the reactant in vapor.
Use for reference its application to microwave device during the reaction, can microwave designing at the auxiliary tool during organic synthesis,
So that the reaction rate of reactant can be greatly speeded up in synthetic reaction process, the time of reaction is reduced, improves combined coefficient,
It saves the energy and reduces the waste of raw material.Publication number is in the utility model patent of CN204911477U, and open one kind can be used for
The organic chemistry apparatus for photoreaction of industrial mass production, while the device is wide, strong applicability with illumination range, carries peace
The characteristics of full protection.But synthetic reaction part has been pertained only to, it is not directed to the further separation and purification treatment to synthetic product, together
The light source of Shi Guangzhao synthetic reactions part does not provide the light of concrete type yet.Or existing organic synthesis solely uses
Illumination or synthesized with heating, be not directed under the conditions of Microwave-assisted synthesis by illumination and heating combine into
The integrated synthetic reaction of row, and synthetic reaction part is to separate progress with product separate section, and operating process can compare
It is complicated, the waste of the energy and test period will certainly be caused.
Utility model content
In order to solve the above technical problems in background technology, with reference to existing organic synthesis technology, this reality
With it is novel start out a kind of new and effective collection illumination synthetic reaction (Xenon light shining), (oil bath pan heating) is reacted in traditional thermal synthesis
And Microwave-assisted synthesis reacts on integrated organic reaction device, can repeatedly be fed intake, synthesis, successive reaction, reality on a small quantity
When detection and analysis, real-time extraction and separation, can also carry out the synthesis and separation of solid product, product liquid and portion gas product,
Not only it had saved the time of organic synthesis but also had reduced the waste of reaction raw materials and the consume of the energy.
To achieve the goals above, the utility model adopts the following technical solution：
A kind of organic chemical synthesis reactor of integration operation, it is characterised in that：The integration operation organises
It includes reaction bulb, reaction bottle cap, reaction bulb heating device, ultrasonic nebulizer, xenon lamp, thermometric and cooling dress to learn synthesis reactor
It sets, extraction equipment, eluent device for formulating, chromatographic column separator and receiving bottle；The reaction bulb is placed on reaction bulb top
Portion is simultaneously closed with reaction bulb；The reaction bulb heating device is placed in reaction bulb bottom and/or side；The ultrasonic nebulizer with it is anti-
It answers and is connected inside bottle；The xenon lamp and thermometric and cooling device are through to from reaction bottle cap inside reaction bulb respectively；It is described
Extraction equipment is arranged in reaction bulb bottom and is connected with inside reaction bulb；The extraction equipment and eluent device for formulating point
It is not connected with chromatographic column separator；The chromatographic column separator is connected with receiving bottle.
Preferably, thermometric and cooling device used by the utility model include thermometer and parallel with thermometer
Condenser pipe；The condenser pipe is straight cold finger；The condenser pipe includes inner tube and the outer tube that is sleeved on outside inner tube；It is described
Cavity is formed between outer tube and inner tube；Water inlet and water outlet are provided on the outer tube；The water inlet by outer tube with
Cavity between inner tube connects with water outlet；Said inner tube includes straight tube and the circular cavity that is arranged on straight tube；It is described
Drier or toxic gas adsorbent are filled in circular cavity.
Preferably, extraction equipment used by the utility model includes being arranged in reaction bulb bottom and mutually being passed through with reaction bulb
Logical extractor；It is provided with liquid taking port on the side wall of the extractor；It is provided with ground glass stopper on the liquid taking port；The extraction
The bottom of device is taken to be connected with chromatographic column separator.
Preferably, extraction equipment used by the utility model further includes syringe；The syringe passes through liquid taking port
Reagent or sampling are added to extractor inside.
Preferably, eluent device for formulating used by the utility model include the first eluant bottle, the first amount fluid cylinder,
Second eluant bottle, the second amount fluid cylinder and eluant, eluent mixed cylinder；First eluant bottle passes through the first amount fluid cylinder and elution
Agent mixed cylinder is connected；Second eluant bottle is connected by the second amount fluid cylinder with eluant, eluent mixed cylinder；The eluant, eluent
Mixed cylinder is connected with chromatographic column separator.
Preferably, eluent device for formulating used by the utility model further includes being placed in inside eluant, eluent mixed cylinder
Electric mixer.
Preferably, chromatographic column separator used by the utility model includes pillar fixed frame and chromatographic column；Institute
State pillar fixed frame include upper grinding port interface bottle stopper, lower ground interface bottle stopper, fixed plate, lift adjustment knob, adjusting rod with
And active plate；The upper grinding port interface bottle stopper and lower ground interface bottle stopper are separately positioned on fixed plate and active plate
On；The chromatographic column be placed between fixed plate and active plate and respectively with upper grinding port interface bottle stopper and lower ground interface bottle
Plug is connected；The lift adjustment knob is connected with active plate by adjusting rod and is driven by adjusting rod to be moved down on active plate
It is dynamic；The extraction equipment and eluent device for formulating respectively be connected at the top of chromatographic column.
Preferably, the organic chemical synthesis reactor of integration operation used by the utility model further includes that setting exists
Microwave generator outside reaction bulb, the drawing liquid pump being placed between reaction bulb and extraction equipment and it is arranged inside reaction bulb
Magnetic stirring apparatus.
Preferably, reaction bulb heating device used by the utility model is oil bath pan or water-bath.
Preferably, the organic chemical synthesis reactor of integration operation used by the utility model further includes concentrating control
Device processed, the central control device include xenon lamp power supply button, xenon lamp brightness regulation knob, oil bath pan power knob, microwave
Device switch button, drawing liquid pump switch button, electric mixer switch button and oil bath pan temperature indicator；The xenon lamp power supply
Button and xenon lamp brightness regulation knob are electrical connected with xenon lamp respectively；The oil bath pan power knob and oil bath pot temperature are aobvious
Show that device is electrical connected with oil bath pan respectively；The microwave device switch button is electrical connected with microwave generator；The drawing liquid pump is opened
Button is closed to be electrical connected with drawing liquid pump；The electric mixer switch button is electrical connected with electric mixer.
The utility model has the advantages that：
The organic chemical synthesis reactor of integration operation provided by the utility model, including it is reaction bulb, reaction bottle cap, anti-
Answer a bottle heating device, ultrasonic nebulizer, xenon lamp, thermometric and cooling device, extraction equipment, eluent device for formulating, chromatographic column point
From device and receiving bottle；Reaction bulb is placed at the top of reaction bulb and closed with reaction bulb；Reaction bulb heating device is placed in reaction
Bottom of bottle portion and/or side；It is connected inside ultrasonic nebulizer and reaction bulb；Xenon lamp and thermometric and cooling device are respectively from reaction
Bottle cap is through to inside reaction bulb；Extraction equipment is arranged in reaction bulb bottom and is connected with inside reaction bulb；Extraction equipment with
And eluent device for formulating is connected with chromatographic column separator respectively；Chromatographic column separator is connected with receiving bottle.
Compared with prior art, it the advantages of the utility model and has the beneficial effect that：
1) the organic chemical synthesis reactor of integration operation provided by the utility model is that collection heating reaction is anti-with illumination
It answers and pillar layer separation is in integrated organic synthesis device, which also can be used alone part instrument, can be according to reality
Test and need voluntarily to select to react required instrument and used, can by the button control reaction process of central control device,
And it can realize and reaction solution is extracted in real time, test and analyze, detach.
2) control button of part instrument is dispersed on central control device, such as the power switch button and brightness tune of xenon lamp
The switch button of section switch, electric mixer switch button, the switch button of oil bath heating device, microwave generator, was tested
Cheng Zhongke completes the experimental implementation of part by controlling these buttons, simple and convenient.
3) raw material of ullrasonic spraying injector, the reaction that can let under superpower ultrasonication can be mixed adequately,
Raw material is entered in the form of fog in the case of being uniformly mixed in reactor again can allow reactant more fully more rapid
Ground participates in reaction, likewise, ultrasonic nebulizer, which is connected to long duct, can be delivered directly to reaction raw materials participation conjunction at xenon lamp
At reaction.
4) connection that round extractor is sealed by the instrument of conduit and upper and bottom section, extractor upper left side
If there are one ground channel and being plugged with ground glass stopper, which is mainly the addition of extractant and inorganic phase in extraction process
Taking-up and thin-layer chromatography analytical sampling provide a channel, meanwhile, which is further equipped with the syringe of different size
It is mainly used for being added and taking out solution.
5) column chromatography for separation part is equipped with special pillar static shelving, sets that there are one lift adjustments to revolve on the right side of shelf
Button can be such that the upper and lower part fixed plate of pillar frame moves a certain distance, can be taken off pillar and carried out to it by turn knob
It promptly replaces and cleans, meanwhile, the upper lower interface on the mouth and pillar frame suitable for reading and lower of pillar is all ground interface, chromatography
The interface caliber size of column and pillar frame has certain specification, and the interface of the two can be sealingly attached to one
It rises, loads onto after chromatographic column that lightly the sealed connection of pillar and pillar frame may be implemented in adjusting knob.The chromatographic column of the part can
For the simple glass chromatographic column of different column diameters and different length, macroporous adsorbent resin chromatography column and organic glass chromatographic column etc.,
Select suitable pillar that can improve the efficiency of pillar layer separation.
6) eluant, eluent that separation process uses can be prepared and can be realized by controlling relevant rotary switch in real time
It is continuous to prepare and continuous use reaches preparation and using integration operation, while the device sets and can prepare and appoint there are two amount fluid cylinder
The eluant, eluent of what ratio, eluant, eluent device for formulating are further equipped with electric mixer and can be stirred after mixing to eluant, eluent
It reuses.
The organic chemical synthesis reactor of integration operation provided by the utility model, both can be in synthetic reaction process
Illumination, can also heat and the participation of microwave radiation technology can allow reaction raw materials rapid and adequately participate in reacting, largely
Accelerating the reaction rate of synthetic reaction makes entire synthesis efficiency be improved, and can be filled by centralized control in experimentation
The button set controls each section reaction condition and reaction process, and realizes and extracted in real time to reaction solution, the thin layer of product
Chromatography, the separation of the rapid preparing of eluant, eluent, chromatographic column.The utility model is intended to combine existing organic synthesis skill
Art, start out a kind of new and effective collection illumination synthetic reaction (Xenon light shining), traditional thermal synthesis reaction (oil bath pan heating) with
And Microwave-assisted synthesis reacts on integrated organic reaction device, which has been provided simultaneously with rapid synthesis and to synthesized product
The integration operation for detaching and purifying in real time is carried out with the mixture of raw material, solid product, product liquid and gas production can be carried out
The separation of object, mainly can repeatedly be fed intake, on a small quantity synthesis, successive reaction and detach in real time, or interruption synthesizes and divides in real time
From etc. experimental implementations.It can also combine one using the part instrument of the device according to specific requirement of experiment in experimentation
Body using whole instrument, control operation is carried out by central control device and the rotary switch of each section in experimentation,
Not only the time of organic synthesis had been saved, but also reduce the waste of reaction raw materials and energy consume, whole operation process to have centainly
Regularity, convenience, have very high practicability.
Description of the drawings
Fig. 1 is the structural schematic diagram of the organic chemical synthesis reactor of integration operation provided by the utility model；
Fig. 2 is the structural schematic diagram of chromatographic column used by the utility model and adjustable pillar fixed frame；
Fig. 3 is the structural schematic diagram with drier condenser pipe used by the utility model；
The reference numerals are as follows：
1- xenon lamp power supply buttons；2- xenon lamp brightness regulation knobs；3- oil bath pan power knobs；4- microwave device switch buttons；
5- drawing liquid pump switch buttons；6- electric mixer switch buttons；7- oil bath pan temperature indicators；8- ultrasonic nebulizers；9- xenon lamps；
10- thermometers；11- condenser pipes；12- the first amount fluid cylinders；The first eluant bottles of 13-；14- electric mixers；The second eluant, eluents of 15-
Bottle；16- the second amount fluid cylinders；17- microwave generators；18- eluant, eluent mixed cylinders；19- drawing liquid pumps；20- pillar fixed frames；21- oil
Bath；22- syringes；23- ground glass stoppers；24- extractors；25- chromatographic columns；26- receiving bottles；27- magnetic stirring apparatus.k、
K1, k2, k3, k4, k5, k6, k7 are the rotary switch of device each section, and k8 is adjusting knob.
Specific implementation mode
In order to be better understood from the above-mentioned technical proposal of the utility model, in the following with reference to the drawings and specific embodiments to this reality
It is described in further detail with novel.
Referring to Fig. 1, the organic chemical synthesis reactor of integration operation provided by the utility model, including centralized control dress
It sets, ullrasonic spraying injector, xenon lamp, thermometer, straight cold finger, microwave generator, oil bath heating device, solvent prepare dress
It sets, electric mixer, magnetic stirring apparatus, air pump, extraction equipment, syringe, chromatographic column, pillar frame and receiving bottle；Ultrasound
The switch of spraying injector is located at its top on ultrasonic nebulizer ontology and is equipped with dress liquid funnel；The switch button and brightness tune of xenon lamp
Section be located at xenon lamp on central control device main function be to provide reaction needed for portion of energy and catalysis accelerate reaction rate；
Head inside straight cold finger carries drier or other impurity removal reagents；The switch button of microwave generator is located at concentration
Microwave mainly plays booster action in synthetic reaction process on control device；Oil bath heating device is equipped with magnetic agitation
It device and shares a switch button with oil bath pan and is all located in central control device operation interface；Eluant, eluent device for formulating mainly leads to
Cross control everywhere two kinds of properties of rotary switch pair eluant, eluent carry out certain volume than real-time mixed preparing；Extraction equipment is furnished with
The syringe of different capabilities, in extraction process using syringe be added organic solvent or distilled water to product and impurity into
Row separating and extracting, the impurity phase being finally obtained by extraction can be taken away with syringe leaves the separation that product carries out next step；Pillar frame
Side has lift adjustment knob that can fix pillar by turn knob and replace pillar, and the upper lower interface of pillar frame is all
The connection that ground interface can be sealed with pillar；Lower interface is all grournd glass in column chromatography and there is sand core in lower end, can root
The chromatographic column of different model is selected to be detached according to the characteristic of separate substance.The control of part instrument is dispersed on central control device
Button processed, as the power switch button and brightness regulating switch of xenon lamp, electric mixer switch button, oil bath heating device are opened
Close the switch button of button, microwave generator.
Input mode is ullrasonic spraying sample introduction, and the raw material for the reaction that can let under ultrasonication can be mixed adequately,
Raw material is entered in the form of fog in the case of being uniformly mixed in reaction unit again can allow reactant more fully and rapid
Ground participate in reaction, ultrasonic nebulizer top be equipped with dress liquid funnel and the right be connected to long duct can be directly defeated by reaction raw materials
It is sent under light source and participates in synthetic reaction.
Xenon lamp has special power switch and intensity of illumination adjusting knob, can experimental specific requirement control xenon lamp
Intensity of illumination, xenon lamp are mounted on to take off at the top of reaction bulb and are cleaned and replaced.Reactor part is equipped with microwave
Device can be manipulated by the switch button of central control device, and the work of auxiliary synthesis is primarily served in synthetic reaction process
With.Drawing liquid pump is internally provided with electric control valve, and the electric control valve and drawing liquid pump share one and switch and be all located at centralized control dress
It sets on interface, waits for extract reaction liquid out by the switch button of central control device after reaction.Thermal response part
Mode of heating be oil bath or water-bath, mode of heating, heater switch and temperature indicator can be voluntarily selected according to requirement of experiment
All it is located at central control device.
The connection that extractor configuration design is sealed at circle and by the instrument of conduit and each section, extractor upper left
Side is set there are one ground channel and being plugged with ground glass stopper, and the addition of extractant and inorganic phase takes predominantly in extraction process
Go out and the analytical sampling of thin-layer chromatography provides a channel, the syringe which is further equipped with different size is mainly used for adding
Enter and take out solution.
Referring to Fig. 2, column chromatography for separation part is equipped with special pillar static shelving, sets that there are one rising-falling tones on the right side of shelf
Knob is saved, the upper and lower part fixed plate of pillar frame can be made to move a certain distance by turn knob, can be taken off pillar to it
Promptly replace and clean, meanwhile, the upper lower interface on the mouth and pillar frame suitable for reading and lower of pillar is all ground interface,
And the interface caliber size of the two has certain specification, load onto after pillar lightly adjusting knob may be implemented pillar with
The sealed connection of pillar frame can select the chromatographic column of variety classes, different column diameters and different length to carry out according to separation requirement
The separation of raw material and product, chromatographic column are internally provided with sand plate.When pillar layer separation detaches raw material with product, used
Eluant, eluent can prepare in real time and can realize continuous prepare and continuous use is realized by controlling relevant rotary switch
It prepares and using integration operation, while the device sets that there are two amount fluid cylinders can prepare the eluant, eluent of any ratio, eluant, eluent
Device for formulating is further equipped with electric mixer and can be stirred to eluant, eluent to be reused after mixing.
Referring to Fig. 3, straight cold finger is internally provided with circular cavity, can be put into drier in circular cavity or have poison gas
Body absorption reagent, while the presence of circular cavity increases and with the contact area of condensed water condensation effect is improved.
Referring to Fig. 1, the utility model provides the organic chemical synthesis reactor of integration operation, including central control device
On control button switch, mainly have xenon lamp power supply button 1, xenon lamp brightness regulation knob 2, oil bath pan power knob 3, microwave device
Switch button 4, drawing liquid pump switch button 5, electric mixer switch button 6, oil bath pan temperature indicator 7, can in experimentation
Experimental implementation is neatly controlled by manipulating these buttons, operating process is simple and convenient.
The organic chemical synthesis reactor installation of integration operation provided by the utility model is provided with light reaction energy
Xenon lamp 9 and thermal response energy provide oil bath pan 21, the device is also equipped with microwave other than both energy-provision way
Device 17 primarily serves the effect of auxiliary in synthetic reaction process.Xenon lamp power supply button 1 can be opened before testing sample introduction
It carries out reaction preheating and the brightness of xenon lamp 9 to be adjusted by xenon lamp brightness regulation knob 2 according to requirement of experiment, then phase again
Synthetic reaction is carried out after pressing oil bath pan power knob 3 and microwave device switch button 4.
The input mode of the organic chemical synthesis reactor of integration operation provided by the utility model is ullrasonic spraying
Sample introduction, reaction before will participate in reaction raw material first mix, be then transferred into the dress liquid funnel on ultrasonic nebulizer 8 and by
Power switch on lower 8 ontology of ultrasonic nebulizer carries out ultrasound, and the raw material mixed liquor in funnel can be in strong ultrasonication therewith
Under gradually form droplet, at this moment open k immediately raw material allowed to be transported to along the long duct on the right side of ultrasonic nebulizer 8 and be placed in reaction
It is reacted around xenon lamp in bottle.
The reaction bulb top of the organic chemical synthesis reactor of integration operation provided by the utility model is respectively provided with
Thermometer 10 and condenser pipe 11, thermometer 10 are used to detect temperature when light reaction carries out, the circular cavity inside condenser pipe 11
It is interior to be put into drier or toxic gas absorption reagent, it can not only play the role of condensation but also dry work can be played
With.
The reaction bulb bottom of the organic chemical synthesis reactor of integration operation provided by the utility model is equipped with pumping
One of electric control valve is equipped in liquid pump 19 and the drawing liquid pump 19, the shared switch button of valve of drawing liquid pump 19 and inside is taken out
It liquid pump switch button 5 and is located on central control device, drawing liquid pump switch button 5 can be pressed after reaction by, which waiting for, to react
Solution afterwards is released from reactor.
The organic chemical synthesis reactor of integration operation provided by the utility model is set to be used for there are one extractor 24
Crude product is extracted, extractor 24 and the drawing liquid pump 19 of upper part are linked together by what conduit sealed, while round
An extraction solution is provided there are one ground glass stopper 23 and the channel of solvent is added and is equipped at the upper left side of extractor
One is the syringe 22 of class specification, the effect of ground glass stopper 23 and syringe 22 be mainly in extraction process extractant plus
Enter the taking-up with inorganic phase and the analytical sampling of thin-layer chromatography, rotary switch k6 can be opened after the completion of processing to be extracted and allows product
As organic phase flows out.
The chromatographic column 25 of the organic chemical synthesis reactor of integration operation provided by the utility model is fixed on pillar
On fixed frame 20, the right side of pillar fixed frame 20 sets that there are one lift adjustment knob k8, can make pillar by turn knob k8
The upper and lower part fixed plate of fixed frame 20 moves a certain distance, and can be taken off chromatographic column 25 and is promptly replaced to it and clearly
It washes, meanwhile, the upper lower interface on the mouth and pillar fixed frame 20 suitable for reading and lower of chromatographic column 25 is all ground interface, and the two
Interface caliber size have certain specification, load onto after pillar that lightly chromatographic column 25 and column may be implemented in adjusting knob k8
The sealed connection of sub- fixed frame 20, at the same the lower section of pillar fixed frame 20 set there are one rotary switch k7 can control solution stream
Go out.
Eluant, eluent can be real used in the organic chemical synthesis reactor of integration operation provided by the utility model
When prepare and can realize continuous prepare and continuous use reach preparation and using one by controlling relevant rotary switch
Change operation, eluant, eluent can be pre-installed in the first eluant bottle 13 and the second eluant bottle 15, then open successively k1 and
Two kinds of reagents of different nature is allowed to enter the first amount fluid cylinder 12 for k2 twice rotary switches and the second amount fluid cylinder 16 measures one respectively
Determine the reagent of volume, following k3 and k4 twice rotary switch allows measured eluent stream then to be pressed to eluant, eluent mixed cylinder 18
Electric mixer switch button 6 allows electric mixer 14 to be stirred the eluant, eluent of two kinds of properties and uses after mixing, should
Device is set there are two the eluant, eluent that amount fluid cylinder can prepare any ratio, and eluant, eluent after mixing can open rotary switch
K5 allows it to flow to chromatography post part and is detached with product as flowing relative raw material, the solution receiving bottle after crossing and detaching
26 receive.
Referring to Fig. 2, chromatographic column separate section used by the utility model includes that chromatographic column and maneuverable pillar are fixed
Frame, the upper lower interface of chromatographic column and the top and the bottom interface that can transfer pillar frame are all grournd glass interfaces, and shelf is upper and lower
Interface caliber size be just consistent with the upper lower interface bore of chromatographic column (i.e. chromatographic column interface can with can transfer pillar bridge joint
Cause for gossip now seals combination).First chromatographic column is loaded in the course of work, then by rotation of adjustment knob adjusting rod is driven
The fixed plate that pillar adds also moves down certain distance, immediately puts on chromatographic column after distance loads onto chromatographic column enough,
Then again lift adjustment knob is recalled to, so that chromatographic column is obtained stable fixation, lift adjustment can be transferred after experiment again
Knob takes out chromatographic column and is replaced and cleaned.
Referring to Fig. 3, straight cold finger used by the utility model is internally provided with circular cavity, can be put in circular cavity
Enter drier or toxic gas absorption reagent, at the same the presence of circular cavity increase make with the contact area of condensed water it is cold
Solidifying effect improves.Straight cold finger can be first cleaned in experimentation and then is put into baking oven, processing is dried, take out drying
Straight cold finger afterwards blocks the lower mouth of circular cavity with absorbent cotton, further according to the corresponding drier of requirement of experiment addition and again
It is blocked with absorbent cotton suitable for reading.Drier after absorbent cotton suitable for reading can be pressed from both sides out with tweezers after testing and then pour out use presss from both sides again
Go out the absorbent cotton of lower mouth, finally entire straight cold finger is started the cleaning processing.
The specific work process of the utility model：Reaction raw materials good in advance will be counted to be ready to and checked each section
The air-tightness of instrument, press xenon lamp power supply button 1 and adjust xenon lamp brightness regulation knob 2 allow xenon lamp 9 shine carry out testing pre- place
Reason, then presses that oil bath pan power knob 3 using oil bath pan 21 heat while magnetic stirring apparatus 27 also begins to rotate, then general
Reaction raw materials are transferred in the funnel on 8 top of ultrasonic nebulizer while turning round lower rotary switch k carries out ultrasound using ultrasonic nebulizer 8
Spraying sample introduction then presses microwave device switch button 4 and microwave generator 17 is allowed to generate microwave radiation technology completion synthetic reaction, light reaction
The temperature of process can be read on thermometer 10, and the temperature of oil bath heating reactive moieties can be in oil bath pan temperature indicator 7
Upper reading, while the condensation and drying of the reaction can be completed in condenser pipe 11.It waits for closing rotation in advance after reaction
Then switch k6 presses drawing liquid pump switch button 5 allows the drawing liquid pump 19 of reaction bulb bottom that reaction liquid is extracted into extractor 24,
Open that water is added into extractor 24 using syringe 22 in the glass stopper on ground glass stopper 23 and organic solvent is extracted again,
Water phase is sucked out with syringe 22 after the completion of to be extracted, remaining organic phase stays in extractor 24, then carries out eluant, eluent
It prepares, eluant, eluent can be pre-installed in the first eluant bottle 13 and the second eluant bottle 15, then open twice rotation successively
It turns on to close k1 and k2 two kinds of reagents of different nature is allowed to enter in the first amount fluid cylinder 12 and the second amount fluid cylinder 16 and measures one respectively
Determining the reagent of volume, following opening twice rotary switch k3 and k4 allow in measured eluent stream to eluant, eluent mixed cylinder 18,
Then pressing electric mixer switch button 6, to allow electric mixer 14 to be stirred the eluant, eluent of two kinds of properties uniformly mixed,
Then chromatographic column 25 is loaded in advance, then makes adjusting rod drive the fixed plate on pillar frame by rotation of adjustment knob k8
Block also moves down certain distance, immediately puts on chromatographic column after distance loads onto chromatographic column enough, then again adjusting knob
K8, which is recalled to, to be come, and chromatographic column is made to obtain stable fixation.Finally opening rotary switch k6 allows the organic phase extracted slowly to drip to
25 top of chromatographic column loaded enables organic matter to be evenly distributed in the layer of silica gel of 25 upper end of chromatographic column, then again
Rotary switch k6 is closed, and is opened rotary switch k5 and is allowed in eluent stream to chromatographic column 25 and carries out chromatography column separation, while
Rotary switch k7 openings receiving bottle 26 is received to the raw material or product flow down together with eluant, eluent.It is closed after the completion of to be separated
Rotary switch k5 and k7 are closed, then rotation of adjustment knob k8 takes out chromatographic column 25 and starts the cleaning processing, and extra eluant, eluent can be with
Rotary switch k5 is beaten next to be utilized again at the upper interface of pillar frame with receiving bottle.
Device provided by the utility model is described in detail below in conjunction with specific embodiment：
The synthesis of sulfamide compound of the embodiment 1 based on arylpyrazole skeleton
Dry 50mL beakers are taken, 4.3g (0.01mol) ethiprole is added into beaker, the acetic acid of 15mL is measured with graduated cylinder
Ethyl ester is poured into beaker, and then weighing 0.48g60%NaH (0.02mol) with pan paper is slowly added in beaker and constantly
Stirring makes it fully dissolve, and then addition 1.9g (0.01mol) continues stirring to benzene sulfonyl chloride makes it be uniformly mixed.Reaction raw materials
Pressing xenon lamp power supply button 1 after being disposed and adjusting xenon lamp brightness regulation knob 2 allows xenon lamp 9 is luminous to carry out experiment pretreatment,
Then press that oil bath pan power knob 3 using oil bath pan 21 heat while magnetic stirring apparatus 27 also begins to rotation and is stirred
Work, then reaction raw materials are transferred in the funnel on 8 top of ultrasonic nebulizer while turning on rotary switch k and utilize ultrasonic nebulizer
8 carry out ullrasonic spraying sample introduction, then press microwave device switch button 4 and the generation 400W microwave radiations of microwave generator 17 is allowed to have assisted
At synthetic reaction, the temperature of light reaction procedure, which is 70~80 DEG C, to be read on thermometer 10, oil bath heating reactive moieties
Temperature, which is 85 DEG C, to be read on oil bath pan temperature indicator 7, and the drier filled in condenser pipe 11 is calcium chloride.It waits reacting
Closing rotary switch k6 after 30min in advance and then pressing drawing liquid pump switch button 5 allows the drawing liquid pump 19 of reaction bulb bottom reaction
Liquid is extracted into extractor 24, then the glass stopper opened on ground glass stopper 23 is added using syringe 22 into extractor 24
The ethyl acetate of 20mL distilled water and 5mL are extracted, and water phase is sucked out with syringe 22 after the completion of to be extracted, remaining organic
It mutually stays in extractor 24, then carries out the preparation of eluant, eluent, ethyl acetate and petroleum ether can be attached separately to first and wash in advance
In de- agent bottle 13 and the second eluant bottle 15, twice rotary switch k1 and k2 are then opened successively and allows ethyl acetate and petroleum ether
It is 1 to respectively enter and measure volume ratio in the first amount fluid cylinder 12 and the second amount fluid cylinder 16 respectively:1 ethyl acetate and petroleum ether,
Next opening k3 and k4 twice rotary switches allows measured ethyl acetate and petroleum ether to flow in eluant, eluent mixed cylinder 18, then
Pressing electric mixer switch button 6, to allow electric mixer 14 to be stirred the eluant, eluent of two kinds of properties uniformly mixed, then
Chromatographic column 25 is loaded in advance, then makes adjusting rod drive the fixed plate on pillar frame by rotation of adjustment knob k8
Certain distance is moved down, is immediately put on chromatographic column after distance loads onto chromatographic column enough, then again adjusting knob k8 tune
Back, chromatographic column is made to obtain stable fixation.Finally opening rotary switch k6 allows the organic phase extracted slowly to drip to
25 top of chromatographic column loaded enables organic matter to be evenly distributed on the silica gel of 25 upper end of chromatographic column, and then rotation is opened again
It closes k6 to close, opens rotary switch k5 and allow and carry out chromatographic column separation in eluent stream to chromatographic column 25, while also by rotary switch
K7 openings receive the raw material or product flow down together with eluant, eluent with receiving bottle 26 and carry out thin-layer chromatographic analysis and collection.
Rotary switch k5 and k7 are closed after the completion of to be separated, then rotation of adjustment knob k8 takes out chromatographic column 25 and starts the cleaning processing, more
Remaining eluant, eluent can beat rotary switch k5 and next be utilized again at the upper interface of pillar frame with receiving bottle.
The photochemical isomers of 2 azobenzene of embodiment is converted and is detached
It takes the anti-azobenzenes of 4g to be dissolved in 30mL anhydrous benzenes, waits for that anti-azobenzene is adequately dissolve in anhydrous benzene, reaction raw materials
Pressing xenon lamp power supply button 1 after being disposed and adjusting xenon lamp brightness regulation knob 2 allows xenon lamp 9 is luminous to carry out experiment pretreatment,
Then press that oil bath pan power knob 3 using oil bath pan 21 heat while magnetic stirring apparatus 27 also begins to rotation and is stirred
Work, then reaction raw materials are transferred in the funnel on 8 top of ultrasonic nebulizer while turning on rotary switch k and utilize ultrasonic nebulizer
8 carry out ullrasonic spraying sample introduction, then press microwave device switch button 4 and the generation 400W microwave radiations of microwave generator 17 is allowed to have assisted
At configuration transfer process, the temperature of light reaction procedure, which is 40~50 DEG C, to be read on thermometer 10, oil bath heating reacting part
The temperature divided, which is 60 DEG C, to be read on oil bath pan temperature indicator 7, and the drier filled in condenser pipe 11 is calcium chloride.It waits for anti-
Closing rotary switch k6 in advance after answering 30min and then pressing drawing liquid pump switch button 5 allows the drawing liquid pump 19 of reaction bulb bottom anti-
Liquid is answered to be extracted into extractor 24, then the glass stopper opened on ground glass stopper 23 extracts one using syringe 22 from extractor 24
Quantitative sample carry out the appearance of the clear product of thin-layer chromatographic analysis and raw material and best eluant, eluent be 3 volume hexamethylenes and
After 1 volume benzene, the preparation of eluant, eluent is then carried out, benzene and hexamethylene can be attached separately to the first eluant bottle 13 and the in advance
In two eluant bottles 15, k1 and k2 twice rotary switch is then opened successively and respectively enters the first amount fluid cylinder 12 by benzene and hexamethylene
And second to measure volume ratio in amount fluid cylinder 16 respectively be 1：Next 3 benzene and hexamethylene is opened the rotation of k3 and k4 twice and is opened
Pass allows in measured benzene and flow of cyclohexane to eluant, eluent mixed cylinder 18, then presses electric mixer switch button 6 and allows electric mixing
It mixes device 14 and the eluant, eluent of two kinds of properties is stirred uniformly mixed, then chromatographic column 25 is loaded in advance, then passes through rotation
Turning adjusting knob k8 makes adjusting rod that the fixed plate on pillar frame be driven also to move down certain distance, when distance is loaded onto enough
Chromatographic column is put on immediately after chromatographic column, then again adjusting knob k8 is recalled to, chromatographic column is made to obtain stable fixation.Finally
Opening rotary switch k6, which allows organic mixture slowly to drip to 25 top of chromatographic column loaded, keeps organic matter uniform
It is distributed on the silica gel of 25 upper end of chromatographic column, then rotary switch k6 is closed again, open rotary switch k5 and eluent stream is allowed to arrive
Chromatographic column separation is carried out in chromatographic column 25, while also receiving rotary switch k7 openings as eluant, eluent flows together with receiving bottle 26
The raw material or product to get off carries out thin-layer chromatographic analysis and collection.Rotary switch k5 and k7 are closed after the completion of to be separated, then
Rotation of adjustment knob k8 takes out chromatographic column 25 and starts the cleaning processing, and extra eluant, eluent can beat rotary switch k5 receiving bottles and exist
It is next utilized again at the upper interface of pillar frame.
The preparation of 3 acetophenone of embodiment with detach
The drying beaker for taking 50mL, weigh 2g adds 10mL anhydrous benzenes through finely ground aluminum trichloride (anhydrous), is stirring
The acetic anhydride of 2mL is slowly added in the process, xenon lamp power supply button 1 is pressed after answering feedstock processing and adjusts xenon lamp brightness tune
Section knob 2 allows xenon lamp 9 to shine and carries out experiment pretreatment, then presses oil bath pan power knob 3 and is heated using oil bath pan 21
Magnetic stirring apparatus 27 also begins to rotation and is stirred work simultaneously, then reaction raw materials are transferred to the leakage on 8 top of ultrasonic nebulizer
Rotary switch k is turned in bucket simultaneously and carries out ullrasonic spraying sample introduction using ultrasonic nebulizer 8, then presses microwave device switch button 4
It allows microwave generator 17 to generate 400W microwave radiations and participates in ancillary synthetic reaction, the temperature of During Illumination is 60 DEG C~70 DEG C or so
It can be read on thermometer 10, the temperature of oil bath heating reactive moieties, which is 100 DEG C, to be read on oil bath pan temperature indicator 7
Go out, the reagent filled in condenser pipe 11 is that calcium oxide particle is used for except the hydrogen chloride gas generated in reaction process.10min to be reacted
Closing rotary switch k6 in advance afterwards and then pressing drawing liquid pump switch button 5 allows the drawing liquid pump 19 of reaction bulb bottom that reaction liquid is taken out
To waiting for that reaction solution is cooled to room temperature in extractor 24, then open glass stopper on ground glass stopper 23 using syringe 22 respectively to
The benzene that 5mL concentrated hydrochloric acids, 10mL ice water and 5mL are injected in extractor 24 is extracted, and nothing is extracted out with syringe 22 after extraction
Machine phase, then extract from extractor 24 a certain amount of sample and carry out the appearance of the clear product of thin-layer chromatographic analysis and raw material and best
The searching of eluant, eluent ratio is the hexamethylene of the benzene and 4 volumes of 1 volume, then carries out the preparation of eluant, eluent, benzene and hexamethylene can
To be attached separately in advance in the first eluant bottle 13 and the second eluant bottle 15, the rotation of k1 and k2 twice is then opened successively and is opened
Pass allow benzene and hexamethylene respectively enter measured respectively in the first amount fluid cylinder 12 and the second amount fluid cylinder 16 volume ratio be 1：4 benzene and
Hexamethylene, following opening k3 and k4 twice rotary switches allow in measured benzene and flow of cyclohexane to eluant, eluent mixed cylinder 18, connect
It and presses electric mixer switch button 6 to allow electric mixer 14 to be stirred the eluant, eluent of two kinds of properties uniformly mixed, connect
It and chromatographic column 25 is loaded in advance, then make adjusting rod drive the fixed plate on pillar frame by rotation of adjustment knob k8
Also certain distance is moved down, is immediately put on chromatographic column after distance loads onto chromatographic column enough, then again adjusting knob k8
It recalls to and, chromatographic column is made to obtain stable fixation.Finally opening rotary switch k6 allows organic mixture slowly to drip to and has filled out
25 top of chromatographic column installed enables organic matter to be evenly distributed on the silica gel of 25 upper end of chromatographic column, then again rotary switch
K6 is closed, and is opened rotary switch k5 and is allowed and carries out chromatographic column separation in eluent stream to chromatographic column 25, while also by rotary switch k7
Opening receives the raw material or product flow down together with eluant, eluent with receiving bottle 26 and carries out thin-layer chromatographic analysis and collection.It waits for
Rotary switch k5 and k7 are closed after the completion of separation, then rotation of adjustment knob k8 takes out chromatographic column 25 and starts the cleaning processing, extra
Eluant, eluent can beat rotary switch k5 and next utilized again at the upper interface of pillar frame with receiving bottle.
Claims (10)
1. a kind of organic chemical synthesis reactor of integration operation, it is characterised in that：The organic chemistry of the integration operation
Synthesis reactor includes reaction bulb, reaction bottle cap, reaction bulb heating device, ultrasonic nebulizer（8）, xenon lamp（9）, thermometric and cooling
Device, extraction equipment, eluent device for formulating, chromatographic column separator and receiving bottle（26）；The reaction bulb is placed on instead
Answer top of bottle and closed with reaction bulb；The reaction bulb heating device is placed in reaction bulb bottom and/or side；The ullrasonic spraying
Device（8）It is connected with inside reaction bulb；The xenon lamp（9）And thermometric and cooling device are through to reaction from reaction bottle cap respectively
Bottle is internal；The extraction equipment is arranged in reaction bulb bottom and is connected with inside reaction bulb；The extraction equipment and elution
Liquid device for formulating is connected with chromatographic column separator respectively；The chromatographic column separator and receiving bottle（26）It is connected.
2. the organic chemical synthesis reactor of integration operation according to claim 1, it is characterised in that：The thermometric and cold
But device includes thermometer（10）And and thermometer（10）Parallel condenser pipe（11）；The condenser pipe（11）It is straight condensation
Pipe；The condenser pipe（11）Including inner tube and the outer tube being sleeved on outside inner tube；Cavity is formed between the outer tube and inner tube；
Water inlet and water outlet are provided on the outer tube；The water inlet passes through the cavity and water outlet phase between outer tube and inner tube
Perforation；Said inner tube includes straight tube and the circular cavity that is arranged on straight tube；In the circular cavity filled with drier or
Toxic gas adsorbent.
3. the organic chemical synthesis reactor of integration operation according to claim 2, it is characterised in that：The extraction dress
It sets including being arranged in reaction bulb bottom and the extractor that connects with reaction bulb（24）；The extractor（24）Side wall on be arranged
There is liquid taking port；It is provided with ground glass stopper on the liquid taking port（23）；The extractor（24）Bottom and chromatography post separation fill
It sets and is connected.
4. the organic chemical synthesis reactor of integration operation according to claim 3, it is characterised in that：The extraction dress
It further includes syringe to set（22）；The syringe（22）By liquid taking port to extractor（24）Inside addition reagent or sampling.
5. the organic chemical synthesis reactor of integration operation according to claim 4, it is characterised in that：The eluent
Device for formulating includes the first eluant bottle（13）, the first amount fluid cylinder（12）, the second eluant bottle（15）, the second amount fluid cylinder（16）With
And eluant, eluent mixed cylinder（18）；First eluant bottle（13）Pass through the first amount fluid cylinder（12）With eluant, eluent mixed cylinder（18）Phase
Connection；Second eluant bottle（15）Pass through the second amount fluid cylinder（16）With eluant, eluent mixed cylinder（18）It is connected；The elution
Agent mixed cylinder（18）It is connected with chromatographic column separator.
6. the organic chemical synthesis reactor of integration operation according to claim 5, it is characterised in that：The eluent
Device for formulating further includes being placed in eluant, eluent mixed cylinder（18）Internal electric mixer（14）.
7. the organic chemical synthesis reactor of integration operation according to claim 6, it is characterised in that：The chromatographic column
Separator includes pillar fixed frame（20）And chromatographic column（25）；The pillar fixed frame（20）Including upper grinding port interface bottle
Plug, lower ground interface bottle stopper, fixed plate, lift adjustment knob, adjusting rod and active plate；The upper grinding port interface bottle stopper
And lower ground interface bottle stopper is separately positioned on fixed plate and active plate；The chromatographic column（25）It is placed in fixed plate
It is connected between active plate and respectively with upper grinding port interface bottle stopper and lower ground interface bottle stopper；The lift adjustment knob is logical
Toning pole is connected with active plate and drives active plate to move up and down by adjusting rod；The extraction equipment and eluent
Device for formulating respectively with chromatographic column（25）Top be connected.
8. according to the organic chemical synthesis reactor of any integration operations of claim 1-7, it is characterised in that：It is described
Organic chemical synthesis reactor further includes the microwave generator being arranged outside reaction bulb（17）, be placed in reaction bulb and extraction equipment
Between drawing liquid pump（19）And the magnetic stirring apparatus being arranged inside reaction bulb（27）.
9. the organic chemical synthesis reactor of integration operation according to claim 8, it is characterised in that：The reaction bulb
Heating device is oil bath pan（21）Or water-bath.
10. the organic chemical synthesis reactor of integration operation according to claim 9, it is characterised in that：The one
The organic chemical synthesis reactor for changing operation further includes central control device, and the central control device includes xenon lamp power supply button
（1）, xenon lamp brightness regulation knob（2）, oil bath pan power knob（3）, microwave device switch button（4）, drawing liquid pump switch button
（5）, electric mixer switch button（6）And oil bath pan temperature indicator（7）；The xenon lamp power supply button（1）And xenon lamp
Brightness regulation knob（2）Respectively with xenon lamp（9）It is electrical connected；The oil bath pan power knob（3）And oil bath pan temperature display
Device（7）Respectively with oil bath pan（21）It is electrical connected；The microwave device switch button（4）With microwave generator（17）It is electrical connected；
The drawing liquid pump switch button（5）With drawing liquid pump（19）It is electrical connected；The electric mixer switch button（6）With electric stirring
Device（14）It is electrical connected.
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| CN201721750699.9U CN207786609U (en) | 2017-12-15 | 2017-12-15 | A kind of organic chemical synthesis reactor of integration operation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107899530A (en) * | 2017-12-15 | 2018-04-13 | 中南民族大学 | A kind of organic chemical synthesis reactor of integration operation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107899530A (en) * | 2017-12-15 | 2018-04-13 | 中南民族大学 | A kind of organic chemical synthesis reactor of integration operation |
| CN107899530B (en) * | 2017-12-15 | 2024-06-11 | 中南民族大学 | Organic chemical synthesis reactor of integration operation |
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